CN108982479A - The luminous device and method for detecting extra large Organic substance in water of ozone chemistry is miniaturized - Google Patents

The luminous device and method for detecting extra large Organic substance in water of ozone chemistry is miniaturized Download PDF

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Publication number
CN108982479A
CN108982479A CN201810646137.2A CN201810646137A CN108982479A CN 108982479 A CN108982479 A CN 108982479A CN 201810646137 A CN201810646137 A CN 201810646137A CN 108982479 A CN108982479 A CN 108982479A
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China
Prior art keywords
ozone
reaction
signal
water
organic substance
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CN201810646137.2A
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Chinese (zh)
Inventor
赵友全
周俊鹏
曹煊
藏鹤超
张密密
宋阳
李振德
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Tianjin University
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Tianjin University
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Application filed by Tianjin University filed Critical Tianjin University
Priority to CN201810646137.2A priority Critical patent/CN108982479A/en
Publication of CN108982479A publication Critical patent/CN108982479A/en
Pending legal-status Critical Current

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/76Chemiluminescence; Bioluminescence

Abstract

The present invention relates to marine environmental monitoring fields, and in particular to micromation ozone chemistry, which shines, detects the device and method of extra large Organic substance in water.The luminous device for detecting extra large Organic substance in water of ozone chemistry is miniaturized, it include: reaction illuminated chamber, injection port at the top of reaction illuminated chamber, ozone inlet positioned at reaction illuminated chamber bottom, the condenser being sequentially connected, optical chamber, photomultiplier tube PMT, photoelectric signal conversion device, driving and signal output cable positioned at reaction illuminated chamber side;The progress of the present invention compared with the existing technology is: the present invention is shortened the gentle path combined of water phase, is expanded the luminous flux of chemiluminescence detection, substantially increase the ability of chemiluminescence detection by the miniature ozone chemistry luminescence-producing reaction device of design.

Description

The luminous device and method for detecting extra large Organic substance in water of ozone chemistry is miniaturized
Technical field:
The present invention relates to marine environmental monitoring fields, and in particular to micromation ozone chemistry, which shines, detects extra large Organic substance in water Device and method.
Background technique:
With economic and science and technology continuous development, the mankind deepen continuously to the exploitation of Yu Haiyang, while the mankind also bring Continuous pollution to ocean, so that marine environment is seriously destroyed.China coastal seas sea area is more universal by organic pollution, And organism kinds in water are more and complicated, and concentration is lower, and the concentration value of different depth difference, so that mostly It is difficult to obtain the organic concentration that can really reflect the sea area in number situation.
The country is mainly at present laboratory measurement to the detection method of organic pollutant in seawater, using alkali formula permanganate The method of oxidimetric titration analyzes to obtain the COD in water, and the major defect of this method is that required time is long, the mistake of analysis Journey is cumbersome, it is desirable that experimental situation it is stringent, required chemical reagent amount is big, and secondary pollution can be generated during detection, small dense Detection accuracy is low equal when spending, and for the chloride ion of such as high concentration of complex environment in seawater, seriously affects testing result.
Summary of the invention:
Object of the present invention is to the luminous device for detecting extra large Organic substance in water of ozone chemistry is miniaturized by chemiluminescence principle And method.
The principle of the present invention: chemoluminescence method by being passed through ozone in the seawater, and the organic molecule in water is in ozone The lower energetic ion for generating excitation state of strong oxidizer effect, it is to release photon-producing chemical hair that unstable ion, which returns ground state, Light.Most of organic compounds such as phenols, short-chain hydrocarbons, fatty acid can generate chemiluminescence in seawater, by collecting spectrum System is collected into photomultiplier tube and is converted into electric signal, by obtaining available having after the signal processings such as subsequent amplification, filtering Machine object content.The specific technical solution of the present invention is as follows:
The luminous device for detecting extra large Organic substance in water of ozone chemistry is miniaturized, comprising: reaction illuminated chamber 3 is located at and reacts hair Injection port 1 at the top of light room, the ozone inlet 2 positioned at reaction illuminated chamber bottom, the successively phase positioned at reaction illuminated chamber side Condenser 5, optical chamber 4, photomultiplier tube PMT6, photoelectric signal conversion device, driving and signal output cable 7 even.
The luminous method for detecting extra large Organic substance in water of the micromation ozone chemistry realized on the above device, including walk as follows It is rapid:
Step 1: opening photoelectric signal conversion device;
Step 2: seawater sample is injected in reaction illuminated chamber by inlet;At the same time, by ozone from ozone air inlet In mouth injection reaction illuminated chamber;
Step 3: while ozone and seawater chemically react, host computer starts simultaneously at signal acquisition, and signal is first fast Speed slowly declines after rising, and start recording when signal rises is accumulated tracer signal until signal no longer declines record end Partite transport is calculated, and signal store and result is calculated by the linear corresponding relation between integrated signal and COD concentration later.
One of preferably, the photoelectric signal conversion device includes: amplifying circuit, filter circuit, ADC modulus turn Change circuit.
Preferably two, the reaction illuminated chamber is cylinder, cylindricality wall surface generally quartz glass.The party The further preferred scheme of case, the reaction illuminated chamber internal coat polytetrafluorethylecoatings coatings, for preventing in tested sample Substance attachment remains in reaction chamber.
Preferably three, further includes: with the sequentially connected throttle valve of injection port, sampling pump, water sample pond, with ozone Air pump that air inlet is sequentially connected, ozone generator, controller, host computer;Described controller one end is connected with air pump, the other end It is connected with host computer;The host computer is also connected with ADC analog to digital conversion circuit.The micromation realized in above-mentioned detection device is smelly The luminous method for detecting extra large Organic substance in water of oxygen chemical, includes the following steps:
Step 1: opening photoelectric signal conversion device;
Step 2: opening sampling pump, throttle valve, extract 3ml seawater sample and injected in reaction illuminated chamber by inlet;Into While entering water sample, host computer issues ozone and generates instruction, and booster air pump after controller is instructed will be in ozone generator Ozone is injected in reaction illuminated chamber by air inlet;
Step 3: while ozone and seawater chemically react, host computer starts simultaneously at signal acquisition, and signal is first fast Speed slowly declines after rising, and start recording when signal rises is accumulated tracer signal until signal no longer declines record end Partite transport is calculated, and signal store and result is calculated by the linear corresponding relation between integrated signal and COD concentration later.
Compared with the existing technology, progress of the invention is: the miniature ozone chemistry luminescence-producing reaction that the present invention passes through design Device shortens the gentle path combined of water phase, expands the luminous flux of chemiluminescence detection, substantially increases chemiluminescence inspection The ability of survey.This method has obtained good implementation result in seawater in the detection of organic humus.
Detailed description of the invention:
Fig. 1 is schematic structural diagram of the device of the invention;In figure, 1 represents injection port, and 2 represent ozone inlet, and 3 represent reaction Illuminated chamber, 4 represent optical chamber, and 5 represent condenser, and 6 represent photomultiplier tube PMT, and 7 represent driving and signal output cable.
Fig. 2 is in embodiment, and sodium humate solution is the signal original graph of water sample;In figure, abscissa represents the reaction time, Unit is the second, and ordinate represents the voltage value that photoelectric detector detects, unit is volt.
Fig. 3 is the linear relationship chart of sodium humate concentration and light intensity integral in embodiment;In figure, abscissa is humic acid Concentration, unit mg/L, ordinate are light intensity integrals.
Specific embodiment:
Embodiment:
The luminous device for detecting extra large Organic substance in water of ozone chemistry is miniaturized, comprising: reaction illuminated chamber 3 is located at and reacts hair Injection port 1 at the top of light room, the ozone inlet 2 positioned at reaction illuminated chamber bottom, the successively phase positioned at reaction illuminated chamber side Even condenser 5, optical chamber 4, photomultiplier tube PMT6, photoelectric signal conversion device, driving and signal output cable 7, with into The sequentially connected throttle valve of sample mouth, sampling pump, water sample pond, the air pump being sequentially connected with ozone inlet, ozone generator, control Device, host computer;Described controller one end is connected with air pump, and the other end is connected with host computer;The host computer also turns with ADC modulus Circuit is changed to be connected;The photoelectric signal conversion device includes: amplifying circuit, filter circuit, ADC analog to digital conversion circuit;It is described anti- Answer illuminated chamber for cylinder, cylindricality wall surface generally quartz glass, outer wall and inner wall are black, dry to reduce reflected light It disturbs, reduces the generation of dark current;The reaction illuminated chamber internal coat polytetrafluorethylecoatings coatings, for preventing in tested sample Substance attachment remains in reaction chamber;The condenser is wide-angle lens, and numerical aperture f/#=4 is sufficiently collected with reaching to meet Chemiluminescence signal purpose.
The luminous method for detecting extra large Organic substance in water of the micromation ozone chemistry realized in above-mentioned detection device, including such as Lower step:
Step 1: opening photoelectric signal conversion device;
Step 2: opening sampling pump, throttle valve, extract 3ml seawater sample and injected in reaction illuminated chamber by inlet;Into While entering water sample, host computer issues ozone and generates instruction, and booster air pump after controller is instructed will be in ozone generator Ozone is injected in reaction illuminated chamber by air inlet;
Step 3: while ozone and seawater chemically react, host computer starts simultaneously at signal acquisition, and signal is first fast Speed slowly declines after rising, and start recording when signal rises is accumulated tracer signal until signal no longer declines record end Partite transport is calculated, and signal store and result is calculated by the linear corresponding relation between integrated signal and COD concentration later.

Claims (7)

  1. The device of extra large Organic substance in water is detected 1. ozone chemistry is miniaturized and shines characterized by comprising reaction illuminated chamber (3), Injection port (1) at the top of reaction illuminated chamber, the ozone inlet (2) positioned at reaction illuminated chamber bottom are located at reaction and shine The condenser (5) being sequentially connected, optical chamber (4), the photomultiplier tube PMT (6), photoelectric signal conversion device, driving of room side With signal output cable (7).
  2. 2. micromation ozone chemistry, which shines, according to claim 1 detects the device of extra large Organic substance in water, which is characterized in that institute Stating photoelectric signal conversion device includes: amplifying circuit, filter circuit, ADC analog to digital conversion circuit.
  3. 3. micromation ozone chemistry, which shines, according to claim 1 detects the device of extra large Organic substance in water, which is characterized in that institute Reaction illuminated chamber is stated as cylinder, cylindricality wall surface generally quartz glass.
  4. 4. micromation ozone chemistry, which shines, according to claim 3 detects the device of extra large Organic substance in water, which is characterized in that institute Reaction illuminated chamber internal coat polytetrafluorethylecoatings coatings are stated, for preventing substance attachment in tested sample, remaining in reaction chamber It is interior.
  5. 5. micromation ozone chemistry, which shines, according to claim 1 detects the device of extra large Organic substance in water, which is characterized in that also Include: and the sequentially connected throttle valve of injection port, sampling pump, water sample pond, the air pump being sequentially connected with ozone inlet, ozone hair Raw device, controller, host computer;Described controller one end is connected with air pump, and the other end is connected with host computer;The host computer also with ADC analog to digital conversion circuit is connected.
  6. The method for detecting extra large Organic substance in water 6. the micromation ozone chemistry realized in claim 1 described device shines, It is characterized in that, includes the following steps:
    Step 1: opening photoelectric signal conversion device;
    Step 2: seawater sample is injected in reaction illuminated chamber by inlet;At the same time, ozone is infused from ozone inlet Enter to react in illuminated chamber;
    Step 3: while ozone and seawater chemically react, host computer starts simultaneously at signal acquisition, and signal is on first quick Slowly decline after rising, tracer signal is carried out integral fortune until signal no longer declines record end by start recording when signal rises It calculates, signal store and result is calculated by the linear corresponding relation between integrated signal and COD concentration later.
  7. 7. the micromation ozone chemistry realized in the detection device described in claim 5, which shines, detects the side of extra large Organic substance in water Method, which comprises the steps of:
    Step 1: opening photoelectric signal conversion device;
    Step 2: opening sampling pump, throttle valve, extract 3ml seawater sample and injected in reaction illuminated chamber by inlet;Into water While sample, host computer issues ozone and generates instruction, booster air pump after controller is instructed, by the ozone in ozone generator It is injected in reaction illuminated chamber by air inlet;
    Step 3: while ozone and seawater chemically react, host computer starts simultaneously at signal acquisition, and signal is on first quick Slowly decline after rising, tracer signal is carried out integral fortune until signal no longer declines record end by start recording when signal rises It calculates, signal store and result is calculated by the linear corresponding relation between integrated signal and COD concentration later.
CN201810646137.2A 2018-06-21 2018-06-21 The luminous device and method for detecting extra large Organic substance in water of ozone chemistry is miniaturized Pending CN108982479A (en)

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CN201810646137.2A CN108982479A (en) 2018-06-21 2018-06-21 The luminous device and method for detecting extra large Organic substance in water of ozone chemistry is miniaturized

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112924439A (en) * 2021-01-29 2021-06-08 山东省科学院海洋仪器仪表研究所 Method for measuring total organic carbon content in water body

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1431485A (en) * 2003-01-30 2003-07-23 山东省科学院海洋仪器仪表研究所 Method for measuring chemistry oxygen consumption of sea water based on luminous intensity principle of ozone oxidation
CN1670509A (en) * 2005-04-28 2005-09-21 国家海洋局第一海洋研究所 Device for detecting chemical oxygen demand in water mass through ozone oxidation-chemoluminescence method
CN1737541A (en) * 2005-08-29 2006-02-22 山东省科学院海洋仪器仪表研究所 Utilize the method for chemiluminescence measurement water body total organic carbon in the ozone oxidation process
CN1865940A (en) * 2006-06-09 2006-11-22 山东省科学院海洋仪器仪表研究所 Method for analyzing water body organism kinds by using ozone chemiluminescence spectrum

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1431485A (en) * 2003-01-30 2003-07-23 山东省科学院海洋仪器仪表研究所 Method for measuring chemistry oxygen consumption of sea water based on luminous intensity principle of ozone oxidation
CN1670509A (en) * 2005-04-28 2005-09-21 国家海洋局第一海洋研究所 Device for detecting chemical oxygen demand in water mass through ozone oxidation-chemoluminescence method
CN1737541A (en) * 2005-08-29 2006-02-22 山东省科学院海洋仪器仪表研究所 Utilize the method for chemiluminescence measurement water body total organic carbon in the ozone oxidation process
CN1865940A (en) * 2006-06-09 2006-11-22 山东省科学院海洋仪器仪表研究所 Method for analyzing water body organism kinds by using ozone chemiluminescence spectrum

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112924439A (en) * 2021-01-29 2021-06-08 山东省科学院海洋仪器仪表研究所 Method for measuring total organic carbon content in water body

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Application publication date: 20181211